JP4913727B2 - 酸素除去触媒および当該触媒を用いた酸素除去方法 - Google Patents
酸素除去触媒および当該触媒を用いた酸素除去方法 Download PDFInfo
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- JP4913727B2 JP4913727B2 JP2007509222A JP2007509222A JP4913727B2 JP 4913727 B2 JP4913727 B2 JP 4913727B2 JP 2007509222 A JP2007509222 A JP 2007509222A JP 2007509222 A JP2007509222 A JP 2007509222A JP 4913727 B2 JP4913727 B2 JP 4913727B2
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- 239000003054 catalyst Substances 0.000 title claims description 246
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- 239000001301 oxygen Substances 0.000 title claims description 57
- 229910052760 oxygen Inorganic materials 0.000 title claims description 57
- 238000000034 method Methods 0.000 title claims description 18
- 239000007789 gas Substances 0.000 claims description 43
- 229910052697 platinum Inorganic materials 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims description 16
- 150000004706 metal oxides Chemical class 0.000 claims description 16
- 239000003638 chemical reducing agent Substances 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 229910052703 rhodium Inorganic materials 0.000 claims description 13
- 229910011214 Ti—Mo Inorganic materials 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 229910006295 Si—Mo Inorganic materials 0.000 claims description 9
- 229910004339 Ti-Si Inorganic materials 0.000 claims description 9
- 229910010978 Ti—Si Inorganic materials 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 229910006774 Si—W Inorganic materials 0.000 claims description 5
- 229910052741 iridium Inorganic materials 0.000 claims description 5
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 10
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- IXSUHTFXKKBBJP-UHFFFAOYSA-L azanide;platinum(2+);dinitrite Chemical compound [NH2-].[NH2-].[Pt+2].[O-]N=O.[O-]N=O IXSUHTFXKKBBJP-UHFFFAOYSA-L 0.000 description 5
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 150000002823 nitrates Chemical class 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 description 3
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- 239000007858 starting material Substances 0.000 description 3
- 150000003609 titanium compounds Chemical class 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- -1 ammine complexes Chemical class 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RSNKHMHUYALIHE-UHFFFAOYSA-N [Mo].[Si].[Ti] Chemical compound [Mo].[Si].[Ti] RSNKHMHUYALIHE-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
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- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 1
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- 239000006193 liquid solution Substances 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- ZPZCREMGFMRIRR-UHFFFAOYSA-N molybdenum titanium Chemical compound [Ti].[Mo] ZPZCREMGFMRIRR-UHFFFAOYSA-N 0.000 description 1
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- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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Description
排ガス中の酸素を除去する。この際の条件については、特に制限はなく、この種の反応に
一般的に用いられている条件で実施することができる。具体的には、排ガスの種類、性状、要求される酸素の除去率などを考慮して適宜決定すればよい。
<触媒調製>
シリカゾル(SiO2として20質量%含有)7.1kgをアンモニア水(NH310質量%含有)140kgと混合した液に、硫酸チタニルの硫酸水溶液(TiO2として125g/リットル、H2SO4として0.55kg/リットル含有)60リットルをよく攪拌しながら徐々に滴下し、沈殿を生成させた。このスラリーを熟成、濾過かつ、洗浄した後、150℃で10時間乾燥した。これを500℃で6時間焼成し、さらにハンマーミルを用いて粉砕し、粉体Aを得た。この粉体Aの平均粒子径は16μmであった。粉体AのX線回折チャートではTiO2やSiO2の明らかな固有ピークは認められず、ブロードな回折ピークによって非晶質な微細構造を有するチタンとケイ素との複合酸化物(Ti−Si複合酸化物)であることが確認された(図2参照)。
上記触媒Aを用いて、下記の条件で酸素除去試験を行った。
酸素:2,000ppm、水素:5,000ppm、窒素:Balance
触媒入口ガス温度:20℃
空間速度:50,000hr−1
反応開始1hr後、触媒処理後のガスをOXYGEN ANALYZERを用いて分析したところ、酸素は検出されなかった。
触媒を市販の一般的なPt−アルミナ−コージェライト触媒(ハニカム型担体、外形150mm角、長さ50mm、目開き1.4mm、肉厚0.4mmにアルミナスラリーを担持させ、その上に白金を担持させてなる触媒)(アルミナ:Pt=98.5:1.5(質量比))に替えた以外は実施例1と同様に酸素除去試験を行った。反応開始1hr後、触媒処理後のガスを分析したところ、酸素を100ppm検出した。
<触媒調製>
メタタングステン酸アンモニウム水溶液(WO3として50質量%含有)12kgをアンモニア水(NH325質量%含有)400kgと水8kgと混合した液に、硫酸チタニルの硫酸水溶液(TiO2として70g/リットル、H2SO4として310g/リットル含有)779リットルをよく攪拌しながら徐々に滴下し、沈殿を生成させた。このスラリーを熟成、濾過、洗浄し、さらに150℃で10時間乾燥した。これを600℃で3時間焼成し、さらにハンマーミルを用いて粉砕し、チタン一夕ングステン混合酸化物粉体B(平均粒子径19μm、Ti−W混合酸化物、TiO2:WO3=90:10(質量比))を得た。この粉体BのX線回折チャートでは、TiO2およびWO3の明らかな固有ピークが2θ=23.5°および2θ=2°にそれぞれ認められた(図3参照)。
上記触媒Bを用いて、下記の条件で酸素除去試験を行った。
酸素:2,000ppm、水素:Balance
触媒入口ガス温度:50℃
空間速度:50,000hr−1
反応開始1hr後、触媒処理後のガスを実施例と同様の方法で分析したところ、酸素は検出されなかった。
<触媒調製>
実施例2で得られた粉体B2kgに成形助剤としての澱粉と水を加え混合し、ニーダーで混練した。得られた混練物にさらに水を加え、ミキサーにてスラリー化し、予め用意したハニカム型コージェライト担体(外形150mm角、長さ50mm、目開き1.4mm、肉厚0.4mm)を浸漬した。その後、該担体を引上げて80℃で乾燥した後、550℃で3時間焼成した。このときのTi−W混合酸化物の担持率は8質量%であった。
上記触媒Cを用いて、下記の条件で酸素除去試験を行った。
酸素:2,000ppm、水素:Balance
触媒入口ガス温度:200℃
空間速度:50,000hr−1
反応開始1hr後、触媒処理後のガスを実施例1と同様の方法で分析したところ、酸素は検出されなかった。
<触媒調製>
アンモニア水(NH325質量%含有)121kgを水86kgと混合した液に、モリブデン酸粉末2.25kgを加え、よく攪拌し、モリブデン酸を完全に溶解させ、均一溶液を調製した。この溶液に硫酸チタニルの硫酸水溶液(TiO2として70g/リットル、H2SO4として287g/リットル含有)257リットルをよく攪拌しながら徐々に滴下し、沈殿を生成させた。このスラリーを熟成、濾過、かつ洗浄し、100℃で10時間乾燥した。これを550℃で4時間焼成し、さらにハンマーミルを用いて粉砕し、チタン−モリブデン混合酸化物粉体C(Ti−Mo混合酸化物、TiO2:MoO3=90:10(質量比))を得た。
上記触媒Dを用いて、下記の条件で酸素除去試験を行った。
酸素:2,000ppm、水素:5,000ppm、二酸化炭素:Balance
触媒入口ガス温度:300℃
空間速度:50,000hr−1
反応開始200hr後、触媒処理後のガスを実施例1と同様の方法で分析したところ、酸素は検出されなかった。
<触媒調製>
シリカゾル(SiO2として30質量%含有)10kgをアンモニア水(NH325質量%含有)101.2kgと水71kgを混合した液に、モリブデン酸粉末2.25kgを加え、よく攪拌し、モリブデン酸を完全に溶解させ、均一溶液を調製した。この溶液に硫酸チタニルの硫酸水溶液(TiO2として70g/リットル、H2SO4として287g/リットル含有)214リットルをよく攪拌しながら徐々に滴下し、沈殿を生成させた。このスラリーを熟成、濾過、かつ洗浄し、100℃で10時間乾燥した。これを550℃で4時間焼成し、さらにハンマーミルを用いて粉砕し、チタン−ケイ素−モリブデン混合酸化物粉体(Ti−Si−Mo混合酸化物、TiO2:SiO2:MoO3=75:15:10(質量比))を得た。
上記触媒Eを用いて、下記の条件で酸素除去試験を行った。
酸素:2,000ppm、水素:Balance
触媒入口ガス温度:400℃
空間速度:50,000hr−1
反応開始200hr後、触媒処理後のガスを実施例1と同様の方法で分析したところ、酸素は検出されなかった。
Claims (16)
- (a)Ti−Mo、(b)Ti−W、(c)Ti−Mo−W、(d)Ti−Si、(e)Ti−Si−Mo、(f)Ti−Si−Wおよび(g)Ti−Si−Mo−Wよりなる群から選ばれた少なくとも1種の複合酸化物または混合酸化物(触媒成分A)およびPt,Pd,RhおよびIrよりなる群から選ばれた少なくとも1種の金属および/またはその金属酸化物(触媒成分B)よりなる酸素除去用触媒。
- 該触媒成分Aおよび該触媒成分Bの合計質量に対して該触媒成分Aが金属酸化物として95〜99.99質量%であり、また該触媒成分Bが金属および/または金属酸化物として5〜0.01質量%である請求項1に記載の触媒。
- 該触媒成分Aが(a)Ti−Mo、(b)Ti−Wおよび(c)Ti−Mo−Wよりなる群から選ばれた少なくとも1種の複合酸化物または混合酸化物である請求項1または2に記載の触媒。
- 該触媒成分Aが(d)Ti−Si、(e)Ti−Si−Mo、(f)Ti−Si−Wおよび(g)Ti−Si−Mo−Wよりなる群から選ばれた少なくとも1種の複合酸化物または混合酸化物である請求項1または2に記載の触媒。
- Tiの含有量が酸化物換算で該触媒成分A全体の50〜99質量%である請求項1〜4のいずれか一つに記載の触媒。
- 該触媒成分Bは、その平均粒子径が0.05〜50nmである請求項1〜5のいずれか一つに記載の触媒。
- 該触媒成分BがPtおよびRhよりなる群から選ばれた少なくとも1種の金属である請求項1〜6に記載の触媒。
- 該触媒成分Aおよび触媒成分Bの合計である該触媒の断面長さをTとした場合に、該触媒の外表面から内部方向に深さT/4の部分にまで存在する該触媒成分Bの量が、該触媒成分の全体量に対して70モル%以上である請求項1〜7のいずれか一つに記載の触媒。
- 該触媒のBET比表面積が30〜250m2/gである請求項1〜8のいずれか一つに記載の触媒。
- 該触媒成分Aおよび触媒成分Bよりなる触媒成分が耐火性無機担体に担持されてなる請求項1〜9のいずれか一つに記載の触媒。
- 該触媒成分Aおよび該触媒成分Bの合計質量に対して該触媒成分Aが金属酸化物として95〜99.9質量%であり、また該触媒成分Bが金属および/または金属酸化物として5〜0.1質量%である請求項1〜10のいずれか一つに記載の触媒。
- 該触媒成分の該耐火性無機担体1リットル当りの担持量が20〜400gである請求項10に記載の触媒。
- 該触媒成分Aの一体成形体に該触媒成分Bを担持してなる請求項1〜9のいずれか一つに記載の触媒。
- 該触媒成分Aおよび該触媒成分Bよりなる触媒成分を一体成形してなる請求項1〜9のいずれか一つに記載の触媒。
- 請求項1〜14のいずれか一つに記載の触媒を用いて還元物質の存在下にガス中の酸素を除去することを特徴とする酸素除去方法。
- 0〜500℃の温度で反応が行われる請求項15に記載の方法。
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PCT/JP2006/305165 WO2006100987A1 (ja) | 2005-03-18 | 2006-03-15 | 酸素除去触媒および当該触媒を用いた酸素除去方法 |
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KR (1) | KR20070112786A (ja) |
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US8366907B2 (en) | 2010-08-02 | 2013-02-05 | Battelle Memorial Institute | Deoxygenation of fatty acids for preparation of hydrocarbons |
EP2611884A4 (en) * | 2010-08-31 | 2014-02-12 | Chevron Usa Inc | MACHINING A HYDROCARBON CIRCULATION |
US8389782B2 (en) * | 2010-08-31 | 2013-03-05 | Chevron U.S.A. Inc. | Biofuel production through catalytic deoxygenation |
US8815085B2 (en) | 2010-09-24 | 2014-08-26 | Chevron U.S.A. Inc. | Process for reducing the total acid number of a hydrocarbon feed |
CN102433183A (zh) * | 2010-09-29 | 2012-05-02 | 中国石油化工股份有限公司 | 常温自启动煤层气脱氧方法 |
CN102433184A (zh) * | 2010-09-29 | 2012-05-02 | 中国石油化工股份有限公司 | 利用氢气直接脱除煤层气中的氧的方法 |
CN102433182A (zh) * | 2010-09-29 | 2012-05-02 | 中国石油化工股份有限公司 | 煤矿区煤层气催化脱氧方法 |
ES2713565T3 (es) | 2011-07-25 | 2019-05-22 | Ilika Tech Ltd | Catalizador de núcleo-cubierta económico con alta estabilidad electroquímica |
CN102553585B (zh) * | 2011-12-23 | 2014-01-15 | 新地能源工程技术有限公司 | 一种用于瓦斯气脱氧的耐硫催化剂及其制备方法和应用 |
CN103071488B (zh) * | 2013-01-09 | 2015-04-01 | 上海化工研究院 | 氢气催化脱氧制备高纯氢用催化剂及其制备方法和应用 |
GB2509916A (en) | 2013-01-16 | 2014-07-23 | Ilika Technologies Ltd | A mixed metal oxide material of tantalum and titanium |
GB201300810D0 (en) | 2013-01-16 | 2013-02-27 | Llika Technologies Ltd | Composite Materials |
GB2509917A (en) * | 2013-01-16 | 2014-07-23 | Ilika Technologies Ltd | Mixed metal oxide materials of titanium and tungsten |
GB2517394A (en) | 2013-01-16 | 2015-02-25 | Ilika Technologies Ltd | Composite materials |
EP2948776B8 (en) | 2013-01-25 | 2020-02-26 | Xcell Biosciences, Inc. | Methods, compositions, kits, and systems for selective enrichment of target cells |
CN105545431B (zh) * | 2015-12-17 | 2017-11-24 | 新昌县鸿吉电子科技有限公司 | 一种车辆尾气净化装置用载体 |
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KR20200097078A (ko) | 2019-02-07 | 2020-08-18 | 주식회사 패러데이오투 | 전기화학적 산소 제거 장치 |
CN112095023B (zh) * | 2020-01-21 | 2022-05-10 | 有研资源环境技术研究院(北京)有限公司 | 一种超亲氧金属-钙协同深度脱除金属锆中氧的方法 |
CN111905837A (zh) * | 2020-07-30 | 2020-11-10 | 成都龙飞科技有限公司 | 一种耐硫脱氧催化剂及其制备方法 |
KR20230057464A (ko) * | 2020-10-08 | 2023-04-28 | 가부시끼가이샤 레조낙 | 산소 분자의 제거 방법 및 일산화탄소의 정제 방법 |
CN115707516B (zh) * | 2021-08-19 | 2024-08-06 | 中国石油化工股份有限公司 | 具有脱氧功能的催化剂和对含氧气的气体进行脱氧的方法 |
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- 2006-03-15 EP EP06729186A patent/EP1859861A1/en not_active Withdrawn
- 2006-03-15 WO PCT/JP2006/305165 patent/WO2006100987A1/ja active Application Filing
- 2006-03-15 JP JP2007509222A patent/JP4913727B2/ja active Active
- 2006-03-15 CN CNA2006800087085A patent/CN101142019A/zh active Pending
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KR20070112786A (ko) | 2007-11-27 |
WO2006100987A1 (ja) | 2006-09-28 |
CN101142019A (zh) | 2008-03-12 |
EP1859861A1 (en) | 2007-11-28 |
US20090041646A1 (en) | 2009-02-12 |
JPWO2006100987A1 (ja) | 2008-09-04 |
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